Epichlorohydrin → HCID 23113189, 화합물

HRID 2355800노트

반응식

HRID 2355800 반응식
[O:1]1[CH2:5][CH2:4][CH2:3]C1.[OH:6][CH2:7][C:8]12[CH2:17][CH:12]3[CH2:13][CH:14]([CH2:16][C:10]([CH2:18][OH:19])([CH2:11]3)[CH2:9]1)[CH2:15]2.[H-].[Na+].[CH2:22]([CH:24]1[O:26][CH2:25]1)Cl>C(Cl)(Cl)Cl>[CH2:22]([O:6][CH2:7][C:8]12[CH2:15][CH:14]3[CH2:13][CH:12]([CH2:11][C:10]([CH2:18][O:19][CH2:3][CH:4]4[O:1][CH2:5]4)([CH2:16]3)[CH2:9]1)[CH2:17]2)[CH:24]1[O:26][CH2:25]1

참가 물질

6

반응물 4

HCID 7835EpichlorohydrinHCID 8028TetrahydrofuranHCID 24758Sodium hydrideHCID 7030111,3-Adamantanedimethanol

생성물 1

HCID 23113189HCID 23113189, 화합물

시약·촉매·용매 1

HCID 6212Chloroform용매

실험 절차

300 ml of dehydrated tetrahydrofuran containing 19.6 g (0.1 mol) of 1,3-bis(hydroxymethyl)adamantane and 5.3 g (0.22 mol) of sodium hydride was stirred in a nitrogen atmosphere at the reflux temperature for 2 hours. Thereto was dropwise added 20.4 g (0.22 mol) of epichlorohydrin, followed by stirring at the reflux temperature for 12 hours. To the reaction mixture was added 200 ml of chloroform, followed by washing with water. The chloroform layer was dried with magnesium sulfate. The dried chloroform layer was subjected to distillation under reduced pressure for solvent removal, whereby was obtained a white solid and oily matter.

후처리

  1. washby washing with water
  2. dry with materialThe chloroform layer was dried with magnesium sulfate
  3. distillationThe dried chloroform layer was subjected to distillation under reduced pressure for solvent removal
  4. customwhereby was obtained a white solid and oily matter

출처 및 근거

ORD 기록
ord-5772540f082e4804b2a7718f9593e7bf
출처 데이터셋
uspto-grants-2010_07
특허 번호
US07754903B2

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